WO2021200394A1 - Batterie rechargeable à électrolyte non aqueux - Google Patents

Batterie rechargeable à électrolyte non aqueux Download PDF

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Publication number
WO2021200394A1
WO2021200394A1 PCT/JP2021/011951 JP2021011951W WO2021200394A1 WO 2021200394 A1 WO2021200394 A1 WO 2021200394A1 JP 2021011951 W JP2021011951 W JP 2021011951W WO 2021200394 A1 WO2021200394 A1 WO 2021200394A1
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Prior art keywords
aqueous electrolyte
group
composite oxide
positive electrode
secondary battery
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PCT/JP2021/011951
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English (en)
Japanese (ja)
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卓司 辻田
圭亮 浅香
基浩 坂田
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パナソニックＩｐマネジメント株式会社
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Priority to JP2022511982A priority Critical patent/JPWO2021200394A1/ja
Priority to US17/913,761 priority patent/US20230099371A1/en
Priority to CN202180025260.2A priority patent/CN115398696A/zh
Publication of WO2021200394A1 publication Critical patent/WO2021200394A1/fr

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
    • H01M10/0566—Liquid materials
    • H01M10/0567—Liquid materials characterised by the additives
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Definitions

  • This disclosure relates to a non-aqueous electrolyte secondary battery.
  • Non-aqueous electrolyte secondary batteries represented by lithium ion secondary batteries have high energy density and high output, and have high energy density and high output, power sources for mobile devices such as smartphones, power sources for vehicles such as electric vehicles, and natural energy such as sunlight. It is promising as a storage device for the energy.
  • a composite oxide containing lithium and a transition metal is used as the positive electrode active material of the non-aqueous electrolyte secondary battery.
  • Patent Document 1 a coating layer containing a metal oxide and a compound containing Li and P is provided on the surface of a composite oxide containing lithium and a transition metal, which is a positive electrode active material of a non-aqueous electrolyte secondary battery. It has been proposed to form.
  • the above metal oxide contains at least one metal element (hereinafter referred to as lanthanoid or the like) selected from the group consisting of groups 3 and 13 of the periodic table and lanthanoids.
  • the compound containing Li and P include Li 3 PO 4 , Li 4 P 2 O 7 , and Li 3 PO 3 (hereinafter, referred to as Li 3 PO 4 and the like).
  • the coating layer is formed by contacting the composite oxide with a raw material solution (a first aqueous solution containing lanthanoids and the like and a second aqueous solution containing P) by a liquid phase method and then heat-treating the composite oxide.
  • the coating layer containing oxides such as lanthanoids and Li 3 PO 4 and the like is formed in an island shape. This is due to the influence of the density difference between the raw material and the product during the heat treatment, the shrinkage of the product, the generation of gas due to the decomposition reaction of the raw material in the raw material solution, and the like.
  • the coating layer is formed in an island shape, the coating of the composite oxide becomes insufficient, and the non-aqueous electrolyte may come into contact with the composite oxide and decompose, resulting in deterioration of cycle characteristics.
  • one aspect of the present disclosure comprises a composite oxide containing lithium and a transition metal and an additive that covers at least a portion of the surface of the composite oxide, wherein the additive is a metal oxidation.
  • the phosphate ester compound comprises a compound and a phosphate ester compound, and the phosphate ester compound relates to a non-aqueous electrolyte secondary battery having at least one alkenyl group in one molecule.
  • the cycle characteristics of the non-aqueous electrolyte secondary battery can be enhanced.
  • FIG. 1 is a schematic perspective view in which a part of the non-aqueous electrolyte secondary battery according to the embodiment of the present disclosure is cut out.
  • the non-aqueous electrolyte secondary battery according to the embodiment of the present disclosure contains a composite oxide (positive electrode active material) containing lithium and a transition metal, and an additive that covers at least a part of the surface of the composite oxide. Be prepared.
  • the additive includes a metal oxide and a phosphoric acid ester compound having at least one alkenyl group in one molecule (hereinafter, also referred to as compound A).
  • the additive that coats the surface of the composite oxide contains a metal oxide and compound A
  • the surface of the composite oxide is sufficiently and stably coated with the additive.
  • decomposition of the non-aqueous electrolyte due to contact with the composite oxide is suppressed, and the cycle characteristics are improved.
  • the surface of the composite oxide is coated in an island shape with the metal oxide, and has a region not covered with the metal oxide.
  • the region not coated with the metal oxide is coated with compound A.
  • metal oxide for example, thickness of 1 nm or more and 5 nm or less
  • compound A improve the coatability of the composite oxide surface with an additive. Therefore, it is possible to avoid the problem that the resistance increases due to the increase in the thickness of the coating layer of the metal oxide by using a large amount of metal oxide in order to improve the coating property.
  • the surface of the composite oxide can be thinly and efficiently coated with a small amount of the metal oxide and the compound A. Therefore, it is easy to obtain a battery having a small internal resistance and excellent cycle characteristics.
  • the alkenyl group (carbon-carbon double bond) of the compound A and the transition metal in the composite oxide Is presumed to be one of the factors for improving the coverage.
  • Compound A is a phosphoric acid ester (organic phosphoric acid) having at least one alkenyl group in one molecule, and compound A can be easily contained by dissolving it in a non-aqueous electrolyte used for a battery.
  • a non-aqueous electrolyte containing compound A can be prepared at the time of battery production, and the surface of the composite oxide can be easily coated with compound A using the non-aqueous electrolyte, which is advantageous in terms of productivity.
  • the carbon-carbon double bond of the alkenyl group is preferably close to the tip of the alkenyl group.
  • Compound A is easily dissolved in the non-aqueous electrolyte, compound A is likely to adhere to the region of the surface of the composite oxide that is not coated with the metal oxide, and the viscosity of the non-aqueous electrolyte containing compound A is adjusted to be appropriately low.
  • the number of carbon atoms of the alkenyl group is preferably 2 or more and 5 or less, for example.
  • the alkenyl group is preferably linear.
  • the plurality of alkenyl groups may be the same as each other or may be different from each other.
  • the alkenyl group consists of a vinyl group, a 1-propenyl group, a 2-propenyl group (allyl group), an isopropenyl group, a 1-butenyl group, a 2-butenyl group and a 3-butenyl group. It may contain at least one selected from the group.
  • Compound A is easily dissolved in the non-aqueous electrolyte, compound A is likely to adhere to the region of the surface of the composite oxide that is not coated with the metal oxide, and the viscosity of the non-aqueous electrolyte containing compound A is adjusted to be appropriately low.
  • the alkenyl group is preferably an allyl group or a 3-butenyl group, and more preferably an allyl group.
  • Compound A has, for example, a structure represented by the following formula (I).
  • R 1 , R 2 and R 3 are alkenyl groups. It is preferable that all of R 1 , R 2 and R 3 are alkenyl groups.
  • the plurality of alkenyl groups may be the same or different from each other.
  • a part of the hydrogen atom contained in the alkenyl group may be replaced with a halogen atom such as a chlorine atom.
  • the number of carbon atoms of the alkenyl group is, for example, 2 or more and 5 or less.
  • the alkenyl group may be linear or branched.
  • R 1 , R 2 and R 3 may be hydrocarbon groups other than alkenyl groups.
  • Hydrocarbon groups other than alkenyl groups include alkyl groups and the like. A part of the hydrogen atom contained in the hydrocarbon group (alkyl group or the like) other than the alkenyl group may be replaced with a halogen atom or the like such as a chlorine atom.
  • the hydrocarbon groups other than the alkenyl group may be the same or different from each other.
  • the number of carbon atoms of the alkyl group is, for example, 2 or more and 5 or less.
  • the alkyl group may be linear or branched.
  • the alkyl group includes a methyl group, an ethyl group, a propyl group and the like.
  • Compound A contains a phosphoric acid monoester, a phosphoric acid diester, and a phosphoric acid triester, and among them, a phosphoric acid triester is preferable.
  • the phosphoric acid triester preferably contains a triallyl phosphate. With a small amount of triallyl phosphate, it is possible to efficiently improve the coverage of the composite oxide whose surface is coated with the metal oxide while suppressing the resistance of the positive electrode to a small value. Further, triallyl phosphate is easily dissolved in a non-aqueous electrolyte, and it is easy to prepare a non-aqueous electrolyte having a low viscosity.
  • the content of compound A in the non-aqueous electrolyte may be 2% by mass or less, 0.25% by mass or more, and 2% by mass or less, based on the total amount of the non-aqueous electrolyte, 0.25. It may be mass% or more and 1.25 mass% or less.
  • the content of compound A may be within the above range at the time of preparation of the non-aqueous electrolyte (before injection into the battery). In this case, the region of the composite oxide surface that is not coated with the metal oxide can be sufficiently coated with the compound A, and the cycle characteristics can be easily improved.
  • the content of Compound A in the preparation of the non-aqueous electrolyte is 2% by mass or less
  • the content of Compound A in the non-aqueous electrolyte in the initial battery (for example, after injecting the non-aqueous electrolyte or after several charges and discharges)
  • the amount may be, for example, 1% by mass or less, 100 ppm or less, or a trace amount close to the detection limit. If the presence of the compound A can be confirmed in the non-aqueous electrolyte in the battery, it is presumed that the compound A derived from the non-aqueous electrolyte is attached to the composite oxide to some extent, and the effect of improving the cycle characteristics corresponding to the compound A is recognized.
  • the content of compound A in the non-aqueous electrolyte is determined by gas chromatography-mass spectrometry (GC / MS) or the like.
  • the metal oxide that coats the surface of the composite oxide does not have a role as a positive electrode active material, unlike the composite oxide used as a positive electrode active material, but has lithium ion conductivity.
  • the metal oxide contains a metal Mc.
  • the metal Mc may contain at least one selected from the group consisting of aluminum, silicon, titanium, magnesium, zirconium, niobium, germanium, calcium and strontium. More specifically, the metal oxide is from the group consisting of aluminum oxide, silicon oxide, titanium oxide, magnesium oxide, zirconium oxide, niobium oxide, germanium oxide, calcium oxide and strontium oxide. It may contain at least one selected.
  • Aluminum oxide includes alumina (Al 2 O 3 ) and the like.
  • the silicon oxide contains silica (SiO 2 ) and the like. Titanium oxide contains TiO 2 and the like. Magnesium oxide includes MgO and the like. Zirconium oxides include ZrO 2 and the like. Further, the metal oxide may include silica alumina (composite oxide containing aluminum and silicon).
  • the metal oxide is a group consisting of aluminum oxide, silicon oxide and silica-alumina from the viewpoint of cost advantage and excellent lithium ion conductivity, chemical stability, and thermal stability. It is preferable to contain at least one selected from the above.
  • the coating amount of the metal oxide can be reduced.
  • the thickness of the metal oxide coating layer can be reduced, for example, in the range of 1 nm or more and 5 nm or less.
  • the thickness of the coating layer of the metal oxide is 5 nm or less, the movement of lithium ions between the composite oxide and the non-aqueous electrolyte through the coating layer of the metal oxide is easy to be carried out smoothly, and the capacity is high and excellent. It is easy to obtain the cycle characteristics.
  • the thickness of the coating layer of the metal oxide may be 1 nm or more and 3 nm or less.
  • the outermost surface of the composite oxide is derived from the metal oxide with respect to Ni derived from the composite oxide.
  • Al atomic ratio: Al / Ni is, for example, 2 or less.
  • a thin layer of the metal oxide for example, a thickness of 1 nm or more and 3 nm or less
  • the distribution state of the metal Mc derived from the metal oxide and the P derived from the compound A is an electron probe microanalyzer (EPMA) or an energy dispersive X-ray (EDX) analyzer for the cross section of the positive mixture layer or the composite oxide. It can be confirmed by performing element analysis (element mapping) using.
  • EPMA electron probe microanalyzer
  • EDX energy dispersive X-ray
  • the positive electrode active material contains a composite oxide containing lithium and a metal Me other than lithium.
  • the metal Me contains at least a transition metal. Transition metals are nickel (Ni), cobalt (Co), manganese (Mn), iron (Fe), copper (Cu), chromium (Cr), titanium (Ti), niobium (Nb), zirconium (Zr), vanadium. It may contain at least one element selected from the group consisting of (V), tantalum (Ta) and molybdenum (Mo).
  • the composite oxide is synthesized by using a coprecipitation method or the like. For example, a lithium compound and a compound containing a metal Me other than lithium obtained by the coprecipitation method or the like are mixed, and the obtained mixture is a predetermined mixture. Obtained by firing under conditions.
  • the composite oxide usually forms secondary particles in which a plurality of primary particles are aggregated.
  • the average particle size (D50) of the composite oxide particles is, for example, 3 ⁇ m or more and 25 ⁇ m or less.
  • the average particle size (D50) of the composite oxide particles means a particle size (volume average particle size) at which the volume integrated value is 50% in the volume-based particle size distribution measured by the laser diffraction scattering method. ..
  • the metal Me may contain a metal other than the transition metal.
  • the metal other than the transition metal may contain at least one selected from the group consisting of aluminum (Al), magnesium (Mg), calcium (Ca), strontium (Sr), zinc (Zn) and silicon (Si). ..
  • the composite oxide may further contain boron (B) and the like in addition to the metal.
  • the transition metal preferably contains at least Ni.
  • the metal Me may contain Ni and at least one selected from the group consisting of Co, Mn, Al, Ti and Fe.
  • the metal Me preferably contains Ni and at least one selected from the group consisting of Co, Mn and Al, and Ni, Co and Mn. And / or Al is more preferred.
  • the metal Me contains Co, the phase transition of the composite oxide containing Li and Ni is suppressed during charging and discharging, the stability of the crystal structure is improved, and the cycle characteristics are likely to be improved.
  • the metal Me contains Mn and / or Al, the thermal stability is improved.
  • the atomic ratio of Ni to the metal Me: Ni / Me may be 0.3 or more and less than 1, preferably 0.5 or more and less than 1. More preferably, it is 0.75 or more and less than 1.
  • the positive electrode active material may contain a composite oxide containing Ni and / or Co, which has a layered rock salt type crystal structure, and has a spinel type crystal structure. It may contain a composite oxide containing Mn. Among them, from the viewpoint of increasing the capacity, a composite oxide having a layered rock salt type crystal structure, containing Ni, and having an atomic ratio of Ni to metal Me: Ni / Me of 0.3 or more (hereinafter, nickel-based composite). It may also be referred to as an oxide).
  • the crystal structure of the nickel-based composite oxide is relatively unstable, and it tends to deteriorate due to the elution of Ni due to the contact with the non-aqueous electrolyte at the high potential positive electrode, and the cycle characteristics tend to deteriorate. Therefore, in the case of the nickel-based composite oxide, the effect of improving the cycle characteristics by coating the composite oxide surface with the additive containing the compound A and the metal oxide can be remarkably obtained. With the above coating, the high capacity of the nickel-based composite oxide can be sufficiently brought out.
  • the composite oxide has a layered rock salt type crystal structure and satisfies the general formula (1): LiNi ⁇ M 1- ⁇ O 2 (0.3 ⁇ ⁇ ⁇ 1, where M is Co, Mn, Al. , Ti and Fe. It is at least one element selected from the group.).
  • ⁇ is in the above range, the effect of Ni and the effect of element M can be obtained in a well-balanced manner.
  • ⁇ may be 0.5 or more, or 0.75 or more.
  • the composite oxide has a crystal structure of the layered rock-salt, and the general formula (2): LiNi x Co y M 1-x-y O It has a composition represented by 2, and in the general formula (2), 0.3 ⁇ x ⁇ 1, 0 ⁇ y ⁇ 0.5 and 0 ⁇ 1-xy ⁇ 0.35 are satisfied, and M is Al and At least one selected from the group consisting of Mn.
  • the x value may be in the range of 0.5 ⁇ x ⁇ 1.
  • the y value may be in the range of 0 ⁇ y ⁇ 0.35.
  • the method of coating the surface of the composite oxide with an additive is, for example, the first step of coating the surface of the composite oxide with the metal oxide and the surface of the composite oxide coated with the metal oxide is coated with the compound A. Including the second step.
  • the first step the surface of the composite oxide is coated with the metal oxide in an island shape, and the surface of the composite oxide has a region not coated with the metal oxide.
  • the second step the region of the surface of the composite oxide that is not coated with the metal oxide is coated with the compound A.
  • a part of the metal oxide may be thinly covered with compound A. Therefore, the surface of the composite oxide is sufficiently coated with the additive containing the metal oxide and the compound A, and the contact between the composite oxide and the non-aqueous electrolyte is sufficiently suppressed.
  • a liquid phase method or a vapor phase method can be used for coating the surface of the composite oxide with the metal oxide in the first step.
  • the liquid phase method include a spray coating method and a dip coating method.
  • the gas phase method include a chemical vapor deposition (CVD) method and an atomic layer deposition (ALD) method.
  • the first step is, for example, a step (1A) of forming a positive electrode mixture layer containing a composite oxide on the surface of a positive electrode current collector, and coating the surface of the positive electrode mixture layer with a metal oxide to form a positive electrode intermediate.
  • the step (1B) of obtaining is included.
  • a positive electrode slurry in which a positive electrode mixture is dispersed in a dispersion medium is applied to the surface of a positive electrode current collector and dried.
  • the dried coating film may be rolled if necessary.
  • the positive electrode mixture layer may be formed on one surface of the positive electrode current collector, or may be formed on both surfaces.
  • the positive electrode mixture contains at least a composite oxide, and may further contain a binder, a conductive agent, and the like.
  • NMP N-methyl-2-pyrrolidone
  • binder examples include resin materials such as fluororesin, polyolefin resin, polyamide resin, polyimide resin, acrylic resin, and vinyl resin.
  • fluororesin examples include polytetrafluoroethylene (PTFE) and polyvinylidene fluoride (PVDF).
  • PTFE polytetrafluoroethylene
  • PVDF polyvinylidene fluoride
  • the conductive agent examples include carbon blacks such as acetylene black; conductive fibers such as carbon fibers and metal fibers; and carbon fluoride.
  • carbon blacks such as acetylene black
  • conductive fibers such as carbon fibers and metal fibers
  • carbon fluoride examples of the conductive agent.
  • one type may be used alone, or two or more types may be used in combination.
  • the positive electrode current collector for example, a metal foil can be used.
  • the metal constituting the positive electrode current collector include aluminum, titanium, alloys containing these metal elements, and stainless steel.
  • the thickness of the positive electrode current collector is not particularly limited, but is, for example, 3 to 50 ⁇ m.
  • step (1B) it is preferable to form a thin layer of metal oxide on the surface of the positive electrode mixture layer by the vapor phase method.
  • the vapor phase method the ALD method is preferable.
  • the coating layer of the metal oxide can be formed thin and island-shaped depending on the temperature at the time of film formation by the ALD method, the amount of the metal oxide deposited, and the like. Even if the coating layer of the metal oxide is formed in an island shape, the coating property of the surface of the composite oxide is enhanced by the compound A in the second step.
  • a raw material gas containing a metal Mc (Al or the like) and an oxidizing agent are alternately supplied to a reaction chamber in which the object is arranged to form a layer containing an oxide of the metal Mc on the surface of the object. It is a film-forming method.
  • the self-limiting action works, so that it is deposited on the surface of the object in atomic layer units. Therefore, the thickness of the metal oxide layer is controlled by the number of cycles in which the supply of the raw material gas ⁇ the exhaust of the raw material gas (purge) ⁇ the supply of the oxidant ⁇ the exhaust of the oxidant (purge) is set as one cycle. That is, the ALD method can easily control the thickness of the formed metal oxide layer.
  • the ALD method can be performed under a temperature condition of 100 to 400 ° C., whereas the CVD is generally performed under a temperature condition of 400 to 900 ° C. That is, the ALD method is excellent in that it can suppress thermal damage to the electrodes.
  • the oxidizing agent used in the ALD method include water, oxygen, ozone and the like.
  • the oxidant may be supplied to the reaction chamber as plasma using the oxidant as a raw material.
  • Al and the like are supplied to the reaction chamber as a precursor gas containing Al and the like.
  • the precursor is, for example, an organometallic compound containing Al or the like, which facilitates chemisorption of Al or the like on an object.
  • organometallic compounds conventionally used in the ALD method can be used.
  • the precursor containing Al include trimethylaluminum ((CH 3 ) 3 Al) and triethylaluminum ((C 2 H 5 ) 3 Al).
  • the surface of the composite oxide is coated with a metal oxide (1a), and the positive electrode mixture layer containing the composite oxide whose surface is coated with the metal oxide is formed on the surface of the positive electrode current collector.
  • (1b) which is a step of forming a positive electrode intermediate and obtaining a positive electrode intermediate, may be included.
  • step (1a) for example, the liquid phase method is used.
  • the step (1a) includes, for example, a step of adhering the raw material solution to the surface of the composite oxide (1a-1) and a step of heating and drying the composite oxide having the raw material solution adhered to the surface (1a-2). include.
  • step (1a-1) for example, a composite oxide is added to the raw material solution and dispersed by stirring.
  • the step (1a-2) is a step of removing the dispersion medium adhering to the surface of the composite oxide by heat drying and reacting the raw materials adhering to the surface of the composite oxide to produce a metal oxide. It also serves as a process.
  • an aqueous solution containing a raw material containing a metal Mc is used.
  • a compound capable of producing a metal oxide by a decomposition reaction by heating can be used, and includes, for example, a metal Mc salt of an organic acid such as citric acid, maleic acid, and lactic acid, and metal Mc. Examples include organic metal complexes.
  • the coating layer of the metal oxide can be formed thin and island-shaped. Even if the coating layer of the metal oxide is formed in an island shape, the coating property of the surface of the composite oxide is enhanced by the compound A in the second step.
  • a positive electrode slurry in which a positive electrode mixture containing a composite oxide whose surface is coated with a metal oxide is dispersed in a dispersion medium is applied to the surface of the positive electrode current collector and dried.
  • the positive electrode mixture may further contain a binder, a conductive agent, and the like.
  • the binder, the conductive agent, the dispersion medium, and the positive electrode current collector those exemplified in the step (1A) may be used.
  • the second step includes a step of preparing a non-aqueous electrolyte containing compound A (2A), a step of contacting the non-aqueous electrolyte containing compound A with a composite oxide whose surface is coated with a metal oxide (2B), and a step of contacting the non-aqueous electrolyte. Is preferably included.
  • step (2B) the region of the surface of the composite oxide that is not coated with the metal oxide is coated with the compound A. Since the compound A is an organic phosphoric acid, the compound A can be easily dissolved and contained in a non-aqueous electrolyte.
  • the surface of the composite oxide can be easily coated with compound A, which is advantageous in terms of improving productivity.
  • an electrode group including a positive electrode intermediate obtained in the step (1B) or the step (1b), a negative electrode, and a separator arranged between the positive electrode intermediate and the negative electrode is configured.
  • the electrode group may contain a non-aqueous electrolyte.
  • the electrode group may be housed in the battery case, the non-aqueous electrolyte may be injected into the battery case containing the electrode group, and the opening of the battery case may be closed with a sealing plate.
  • the surface of the positive electrode mixture layer coated with the metal oxide can be further coated with the compound A by the step (2B).
  • the surface of the composite oxide coated with the metal oxide can be further coated with the compound A by the step (2B). Since the coating with the compound A is performed after the formation of the positive electrode mixture layer, it is easy to form contacts between the composite oxide particles without interposing the compound A, and it is easy to secure a conductive network between the composite oxide particles.
  • the positive electrode may include, for example, a positive electrode current collector, a positive electrode mixture layer supported on the surface of the positive electrode current collector, and a positive electrode mixture layer containing at least a composite oxide.
  • the positive electrode mixture layer may further contain the above-mentioned conductive agent, binder and the like.
  • the surface of the composite oxide contained in the positive electrode mixture layer may be coated with an additive containing a metal oxide and compound A.
  • the surface of the positive electrode mixture layer containing the composite oxide may be coated with an additive containing a metal oxide and compound A.
  • the negative electrode may include a negative electrode current collector and a negative electrode mixture layer supported on the surface of the negative electrode current collector.
  • the negative electrode mixture layer can be formed, for example, by applying a negative electrode slurry in which a negative electrode mixture is dispersed in a dispersion medium to the surface of a negative electrode current collector and drying it. The dried coating film may be rolled if necessary.
  • the negative electrode mixture layer may be formed on one surface of the negative electrode current collector, or may be formed on both surfaces.
  • the dispersion medium for example, water or NMP is used.
  • the negative electrode mixture contains a negative electrode active material as an essential component, and may contain a binder, a conductive agent, a thickener, and the like as optional components.
  • a binder and the conductive agent those exemplified for the positive electrode can be used.
  • a rubber material such as styrene-butadiene copolymer rubber (SBR) may be used as the binder.
  • SBR styrene-butadiene copolymer rubber
  • the thickener include carboxymethyl cellulose (CMC) and a modified product thereof (Na salt, etc.).
  • the negative electrode active material may contain a carbon material that occludes and releases lithium ions.
  • Examples of the carbon material that occludes and releases lithium ions include graphite (natural graphite, artificial graphite), easily graphitized carbon (soft carbon), and non-graphitized carbon (hard carbon). Of these, graphite is preferable because it has excellent charge / discharge stability and has a small irreversible capacity.
  • the negative electrode active material may contain an alloy-based material.
  • the alloy-based material is a material containing at least one kind of metal capable of forming an alloy with lithium, and examples thereof include silicon, tin, silicon alloys, tin alloys, and silicon compounds.
  • silicon compound a composite material including a lithium ion conductive phase and silicon particles dispersed in the phase may be used.
  • a silicate phase such as a lithium silicate phase, a silicon oxide phase in which 95% by mass or more is silicon dioxide, a carbon phase, or the like may be used.
  • An alloy material and a carbon material may be used in combination as the negative electrode active material.
  • the ratio of the carbon material to the total of the alloy-based material and the carbon material is, for example, preferably 80% by mass or more, and more preferably 90% by mass or more.
  • the shape and thickness of the negative electrode current collector can be selected from the shape and range according to the positive electrode current collector.
  • the metal constituting the negative electrode current collector include copper (Cu), nickel (Ni), iron (Fe), and alloys containing these metal elements.
  • the non-aqueous electrolyte contains a non-aqueous solvent and a lithium salt dissolved in the non-aqueous solvent.
  • the non-aqueous electrolyte may contain compound A.
  • the compound A contained in the non-aqueous electrolyte may be attached to the surface of the composite oxide, and the surface of the composite oxide may be coated with the compound A.
  • the concentration of the lithium salt in the non-aqueous electrolyte is preferably, for example, 0.5 mol / L or more and 2 mol / L or less. By controlling the lithium salt concentration within the above range, a non-aqueous electrolyte having excellent ionic conductivity and appropriate viscosity can be obtained.
  • the lithium salt concentration is not limited to the above.
  • cyclic carbonate ester for example, cyclic carbonate ester, chain carbonate ester, cyclic carboxylic acid ester, chain carboxylic acid ester and the like are used.
  • the cyclic carbonate include propylene carbonate (PC) and ethylene carbonate (EC).
  • the cyclic carbonate may include a fluorinated cyclic carbonate such as fluoroethylene carbonate (FEC) or a cyclic carbonate having a carbon-carbon unsaturated bond such as vinylene carbonate (VC) or vinylethylene carbonate.
  • chain carbonic acid ester include diethyl carbonate (DEC), ethyl methyl carbonate (EMC), dimethyl carbonate (DMC) and the like.
  • Examples of the cyclic carboxylic acid ester include ⁇ -butyrolactone (GBL) and ⁇ -valerolactone (GVL).
  • Examples of the chain carboxylic acid ester include methyl formate, ethyl formate, propyl formate, methyl acetate, ethyl acetate, propyl acetate, methyl propionate, ethyl propionate, propyl propionate and the like.
  • the non-aqueous solvent one type may be used alone, or two or more types may be used in combination.
  • lithium salt a known lithium salt can be used.
  • Preferred lithium salts include, for example, LiClO 4 , LiBF 4 , LiPF 6 , LiAlCl 4 , LiSbF 6 , LiSCN, LiCF 3 SO 3 , LiCF 3 CO 2 , LiAsF 6 , LiB 10 Cl 10 , lower aliphatic lithium carboxylate, and the like.
  • Examples thereof include LiCl, LiBr, LiI, borates and imide salts.
  • borates include bis (1,2-benzenediorate (2-) -O, O') lithium borate and bis (2,3-naphthalenedioleate (2-) -O, O') boric acid.
  • imide salts include lithium bis (fluorosulfonyl) imide (LiN (FSO 2 ) 2 ), imidelithium bistrifluoromethanesulfonate (LiN (CF 3 SO 2 ) 2 ), and imidelithium nonafluorobutanesulfonate trifluoromethanesulfonate.
  • lithium bispentafluoroethanesulfonate LiN (C 2 F 5 SO 2 ) 2
  • LiN (C 2 F 5 SO 2 ) 2 imid lithium bispentafluoroethanesulfonate
  • One type of lithium salt may be used alone, or two or more types may be used in combination.
  • the separator may contain a non-aqueous electrolyte containing compound A.
  • the separator has high ion permeability and has appropriate mechanical strength and insulation.
  • a microporous thin film, a woven fabric, a non-woven fabric or the like can be used.
  • polyolefins such as polypropylene and polyethylene are preferable.
  • Non-aqueous electrolyte secondary battery is a structure in which an electrode group in which a positive electrode and a negative electrode are wound via a separator and a non-aqueous electrolyte are housed in an exterior body.
  • an electrode group in which a positive electrode and a negative electrode are wound via a separator and a non-aqueous electrolyte are housed in an exterior body.
  • another form of electrode group such as a laminated type electrode group in which a positive electrode and a negative electrode are laminated via a separator may be applied.
  • the non-aqueous electrolyte secondary battery may be in any form such as a cylindrical type, a square type, a coin type, a button type, and a laminated type.
  • FIG. 1 is a schematic perspective view in which a part of the non-aqueous electrolyte secondary battery according to the embodiment of the present disclosure is cut out.
  • the battery includes a bottomed square battery case 4, an electrode group 1 housed in the battery case 4, and a non-aqueous electrolyte.
  • the electrode group 1 has a long strip-shaped negative electrode, a long strip-shaped positive electrode, and a separator that is interposed between them and prevents direct contact.
  • the electrode group 1 is formed by winding a negative electrode, a positive electrode, and a separator around a flat plate-shaped winding core and pulling out the winding core.
  • One end of the negative electrode lead 3 is attached to the negative electrode current collector of the negative electrode by welding or the like.
  • the other end of the negative electrode lead 3 is electrically connected to the negative electrode terminal 6 provided on the sealing plate 5 via a resin insulating plate.
  • the negative electrode terminal 6 is insulated from the sealing plate 5 by a resin gasket 7.
  • One end of the positive electrode lead 2 is attached to the positive electrode current collector of the positive electrode by welding or the like.
  • the other end of the positive electrode lead 2 is connected to the back surface of the sealing plate 5 via an insulating plate. That is, the positive electrode lead 2 is electrically connected to the battery case 4 that also serves as the positive electrode terminal.
  • the insulating plate separates the electrode group 1 and the sealing plate 5, and also separates the negative electrode lead 3 and the battery case 4.
  • the peripheral edge of the sealing plate 5 is fitted to the open end portion of the battery case 4, and the fitting portion is laser welded. In this way, the opening of the battery case 4 is sealed with the sealing plate 5.
  • the non-aqueous electrolyte injection hole provided in the sealing plate 5 is closed by the sealing 8.
  • NMP N-Methyl-2-pyrrolidone
  • AB acetylene black
  • PVDF polyvinylidene fluoride
  • the positive electrode active material layered rock salt type composite oxide particles having a composition of LiNi 0.35 Co 0.35 Mn 0.30 (NCM) (average particle size (D50) 4 ⁇ m) were used.
  • NCM LiNi 0.35 Co 0.35 Mn 0.30
  • a positive electrode slurry was applied to the surface of the aluminum foil, the coating film was dried, and then rolled to form a positive electrode mixture layer.
  • the positive electrode mixture layer was formed on both sides of the aluminum foil. Further, the surface of the positive electrode mixture layer was coated with Al 2 O 3 by the ALD method (temperature: 120 ° C., precursor: trimethylaluminum, oxidizing agent: H 2 O, pressure: several Torr, 10 cycles). In this way, a positive electrode intermediate was obtained.
  • the atomic ratio Al / Ni on the outermost surface of the positive electrode intermediate determined by the method described above was 2 or less.
  • a negative electrode slurry Water was added to the negative electrode mixture and stirred to prepare a negative electrode slurry.
  • a mixture of artificial graphite (average particle size 20 ⁇ m), styrene-butadiene rubber (SBR), and sodium carboxymethyl cellulose (CMC-Na) was used.
  • the mass ratio of artificial graphite, SBR, and CMC-Na was 100: 1: 1.
  • a negative electrode slurry was applied to the surface of the copper foil, the coating film was dried, and then rolled to prepare a negative electrode having a negative electrode mixture layer formed on both sides of the copper foil.
  • LiPF 6 was dissolved in a mixed solvent (volume ratio 2: 8) of fluoroethylene carbonate (FEC) and dimethyl carbonate (DMC), and triallyl phosphate (TP) was further added to obtain a non-aqueous electrolyte.
  • the concentration of LiPF 6 in the non-aqueous electrolyte was 1 mol / L.
  • the content of TP in the non-aqueous electrolyte was set to the value shown in Table 1.
  • a positive electrode lead made of Al was attached to the positive electrode intermediate obtained above.
  • a negative electrode lead made of Ni was attached to the negative electrode obtained above.
  • the positive electrode intermediate and the negative electrode were spirally wound through a polyethylene thin film (separator) to prepare a wound electrode group.
  • the electrode group was housed in a bag-shaped exterior body formed of a laminated sheet provided with an Al layer, and after injecting the above-mentioned non-aqueous electrolyte, the exterior body was sealed to prepare a non-aqueous electrolyte secondary battery.
  • the positive electrode intermediate was brought into contact with the non-aqueous electrolyte solution (TP) in the battery, and the surface of the positive electrode mixture layer was further coated with TP to obtain a positive electrode.
  • TP non-aqueous electrolyte solution
  • the batteries of Examples 1 to 4 are A1 to A4, respectively.
  • Comparative Example 2 In the preparation of the non-aqueous electrolyte, the battery B2 was produced by the same method as that of the battery A1 of Example 1 except that the non-aqueous electrolyte did not contain TP.
  • the batteries A1 to A4 had a higher capacity retention rate than the batteries B1 to B3.
  • the battery B1 since the surface of the positive electrode mixture layer was not coated with either Al 2 O 3 or TP, the non-aqueous electrolyte and the composite oxide came into contact with each other, and the capacity retention rate decreased.
  • the surface of the positive electrode mixture layer was coated with Al 2 O 3 , but since it was not coated with TP, the coating of the positive electrode mixture layer was insufficient, and the non-aqueous electrolyte and the composite oxide came into contact with each other. The capacity retention rate has decreased.
  • the surface of the positive electrode mixture layer was coated with TP, but was not coated with Al 2 O 3 , so that the internal resistance (the resistance of the positive electrode) increased and the capacity retention rate decreased.
  • the battery A3 has a higher TP content than the battery B3, but since the surface of the positive electrode mixture layer is coated with Al 2 O 3 , the internal resistance (positive electrode resistance) is reduced as compared with the battery B3.
  • the non-aqueous electrolyte secondary battery according to the present disclosure is suitably used, for example, as a power source for mobile devices such as smartphones, a power source for vehicles such as electric vehicles, and a storage device for natural energy such as sunlight.
  • Electrode group 2 Positive electrode lead 3 Negative electrode lead 4 Battery case 5 Seal plate 6 Negative terminal 7 Gasket 8 Seal

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Abstract

Cette batterie rechargeable à électrolyte non aqueux comprend une électrode positive, une électrode négative et un électrolyte non aqueux. L'électrode positive est pourvue d'un oxyde complexe contenant du lithium et d'un métal de transition, et d'un additif qui recouvre au moins une partie de la surface de l'oxyde complexe. L'additif contient un oxyde métallique, et un composé ester d'acide phosphorique, le composé ester d'acide phosphorique ayant au moins un groupe alcényle dans une molécule unique.
PCT/JP2021/011951 2020-03-31 2021-03-23 Batterie rechargeable à électrolyte non aqueux WO2021200394A1 (fr)

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WO2022163579A1 (fr) * 2021-01-29 2022-08-04 パナソニックＩｐマネジメント株式会社 Batterie secondaire à électrolyte non aqueux et son procédé de fabrication
US11502300B1 (en) * 2021-10-13 2022-11-15 Shenzhen Capchem Technology Co., Ltd. Secondary battery
WO2022259797A1 (fr) * 2021-06-11 2022-12-15 パナソニックＩｐマネジメント株式会社 Matière active d'électrode positive revêtue, matériau d'électrode positive, et batterie
WO2023169096A1 (fr) * 2022-03-10 2023-09-14 宁德时代新能源科技股份有限公司 Matériau actif d'électrode positive, batterie secondaire, module de batterie, bloc-batterie et dispositif électrique
WO2024142770A1 (fr) * 2022-12-26 2024-07-04 パナソニックＩｐマネジメント株式会社 Matériau actif d'électrode positive revêtu, électrode positive et batterie secondaire

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JP2019536194A (ja) * 2016-11-25 2019-12-12 シェンズェン カプチェム テクノロジー カンパニー リミテッドＳｈｅｎｚｈｅｎ Ｃａｐｃｈｅｍ Ｔｅｃｈｎｏｌｏｇｙ Ｃｏ．， Ｌｔｄ． リチウムイオン電池

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JP2019536194A (ja) * 2016-11-25 2019-12-12 シェンズェン カプチェム テクノロジー カンパニー リミテッドＳｈｅｎｚｈｅｎ Ｃａｐｃｈｅｍ Ｔｅｃｈｎｏｌｏｇｙ Ｃｏ．， Ｌｔｄ． リチウムイオン電池

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Publication number Priority date Publication date Assignee Title
WO2022163579A1 (fr) * 2021-01-29 2022-08-04 パナソニックＩｐマネジメント株式会社 Batterie secondaire à électrolyte non aqueux et son procédé de fabrication
WO2022259797A1 (fr) * 2021-06-11 2022-12-15 パナソニックＩｐマネジメント株式会社 Matière active d'électrode positive revêtue, matériau d'électrode positive, et batterie
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WO2023169096A1 (fr) * 2022-03-10 2023-09-14 宁德时代新能源科技股份有限公司 Matériau actif d'électrode positive, batterie secondaire, module de batterie, bloc-batterie et dispositif électrique
WO2024142770A1 (fr) * 2022-12-26 2024-07-04 パナソニックＩｐマネジメント株式会社 Matériau actif d'électrode positive revêtu, électrode positive et batterie secondaire

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